EP0018068B1 - Adjustable vapour deposition apparatus - Google Patents

Adjustable vapour deposition apparatus Download PDF

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Publication number
EP0018068B1
EP0018068B1 EP80300618A EP80300618A EP0018068B1 EP 0018068 B1 EP0018068 B1 EP 0018068B1 EP 80300618 A EP80300618 A EP 80300618A EP 80300618 A EP80300618 A EP 80300618A EP 0018068 B1 EP0018068 B1 EP 0018068B1
Authority
EP
European Patent Office
Prior art keywords
reservoir
reservoirs
vapor
vapor deposition
reaction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP80300618A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0018068A1 (en
Inventor
Michael Gregg Blankenship
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corning Glass Works
Original Assignee
Corning Glass Works
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Corning Glass Works filed Critical Corning Glass Works
Priority to AT80300618T priority Critical patent/ATE10292T1/de
Publication of EP0018068A1 publication Critical patent/EP0018068A1/en
Application granted granted Critical
Publication of EP0018068B1 publication Critical patent/EP0018068B1/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01413—Reactant delivery systems
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4485—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/04—Multi-nested ports
    • C03B2207/06—Concentric circular ports
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/04—Multi-nested ports
    • C03B2207/12—Nozzle or orifice plates
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/80—Feeding the burner or the burner-heated deposition site
    • C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/80—Feeding the burner or the burner-heated deposition site
    • C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
    • C03B2207/87—Controlling the temperature

Definitions

  • the present invention relates to glass producing apparatus, and more particularly to improved means for supplying vaporized source material to an apparatus for forming blanks to be drawn into optical waveguides.
  • Light can be caused to propagate within an elongate transparent body (such as a filament of glass or the like) in discrete modes if certain preconditions are met.
  • the size of the filament, the radial gradation in refractive index, and other considerations combine to determine the effectiveness of the filament as a transmitting medium for optical communications.
  • the internal characteristics of the strand must be closely controlled.
  • a filament suitable for use as an optical waveguide can be formed by heating a cylindrical blank of a transparent dielectric material, such as glass, and drawing the blank into the desired thin, elongate structure.
  • the structural characteristics of the waveguide closely reflect those of the blank from which it is drawn, particularly the gradient of the refractive index.
  • a drawing blank is formed by coating a rotating, cylindrical starting member with successive layers of a suitable sinterable glass soot.
  • the soot is built up, layer by layer, from minute siliceous particles which are applied to the surface of the blank through the mechanism of an oxidizing reaction flame or the like.
  • the flame used for sintering and transferring particles to the surface of a glass blank or the like has in the past been termed a "hydrolyzing flame".
  • siliceous matrix material such as silicon tetrachoride
  • dopants are also supplied in controlled amounts and at particular times to vary the optical characteristics of the end product. It should be understood that whereas the preferred embodiment is described in conjunction with the formation of silicate glasses, silica-free glasses containing ger- mania for example, may be formed by the apparatus of this invention.
  • the vaporous source material is directed into a heated tube.
  • the material is deposited within the tube in successive layers and the tube is then collapsed to leave a fused blank.
  • the blank is subsequently heated and drawn into an elongate filament.
  • US-A-4062665 discloses a vapor deposition apparatus for forming an optical waveguide blank, comprising at least two reservoirs containing liquid source materials, heating means for each reservoir, reaction means for forming a reaction product, piping for supplying reagent vapors and optionally carrier gas from said reservoirs to said reaction means and a respective metering means located in the piping extending between each reservoir and said reaction means, the metering means being in the form of a flow control valve in the piping at the output of each reservoir, each said valve having a mechanism to effect valve adjustment.
  • the reservoirs are housed in constant temperature baths to maintain the liquid compositions at the desired temperatures, thereby holding their vapor pressures constant.
  • Our copending United Kingdom Patent Application No. A 2015991 discloses an apparatus which supplies a precisely controlled amount of reactant vapors to discharge means.
  • various reaction product constituents are maintained in liquid form in reservoirs, and a metering pump is coupled to each reservoir for delivering a predetermined volume of the liquid constituent to a mixing stage.
  • the various liquids are thoroughly mixed, then nebulized.
  • the material vapors are transported to discharge means such as a reaction burner or the like.
  • the source material vapors are then reacted in the flame in a conventional manner, and deposited upon a substrate to form a product such as an optical waveguide blank.
  • the apparatus of the said copending United Kingdom Patent Application is capable of precisely controlling the amount of the various reaction product constituents delivered to the utilization means, the variable output pumps utilized in that apparatus are very expensive.
  • vapor deposition apparatus for forming an optical waveguide blank, comprising at least two reservoirs containing liquid source materials, heating means for each reservoir, reaction means for forming a reaction product, piping for supplying reagent vapors but no carrier gas from said reservoirs to said reaction means and a respective metering means located in the piping extending between each reservoir and said reaction means, the metering means being in the form of a flow control valve in the piping at the output of each reservoir, each said valve having a mechanism to effect valve adjustment, characterized in that the reservoir heating means for each reservoir comprises means for sensing the vapor pressure within each said reservoir and means responsive to a signal generated by said pressure sensing means for supplying to each of said reservoirs an amount of heat necessary to heat the liquid source materials in the reservoirs to a temperature sufficient to convert the liquid source materials therein to a vapor of predetermined minimum vapor pressure within each reservoir, said heating means being such that the vapor pressure within each reservoir does not remain constant but may rise above said minimum vapor pressure.
  • a layer of glass soot is applied to a substantially cylindrical mandrel or starting member 10 by discharge means such as a flame hydrolysis burner 12.
  • the starting member is rotated and translated with respect to the burner so as to build up a generally cylindrical preform 16.
  • the present illustration is described in connection with the formation of the blank susceptible of being drawn into an optical waveguide, although the invention is not necessarily limited to such applications.
  • the substrate or starting member 10 can subsequently be removed by mechanical or chemical processes so as to leave only the deposited material.
  • the cylindrical blank is subsequently drawn into an elongate waveguide whose characteristics reflect the composition of the reaction product constituents.
  • techniques other than flame reaction may be chosen for depositing the desired reaction products.
  • the reaction of vapors may take place within a heated region of a substrate tube, deposition of glass occurring on the inner surface of the tube, a process sometimes referred to as inside vapor phase oxidation (IVPO).
  • IVPO inside vapor phase oxidation
  • the constituents which are ultimately incorporated in the reaction products are maintained in reservoirs 18, 20 and 22 which may be commercially-available pressurized tanks. These reservoirs are provided with heaters 24, 2.6 and 28 for maintaining the temperature of the reactants sufficiently high to maintain the vapor pressure within the reservoirs at a level sufficient to cause adequate vapor flow through the metering apparatus to the burner.
  • the minimum vapor pressure for accomplishing this purpose is 4 psig (27 x 10 3 Pascals gauge).
  • the maximum pressure in the reservoirs is dictated by equipment limitations such as the mass flow controller described hereinbelow, the recommended maximum operating pressure of which is 150 psig (1.0 x 10 6 Pascals gauge).
  • Temperature controllers 30, 32, 34 which maintain the source material in each reservoir at an appropriate temperature, may be selected from such commercially available units as model 383 Robert Shaw controllers, Eurotherm controllers, or the like.
  • Pressure sensors 36, 38 and 40 provide controllers 30, 32 and 34, respectively, with control signals. Accordingly, the reservoir pressure is monitored, and the information thus derived is used to control the operation of heaters 24, 26 and 28.
  • Appropriate valves 42, 44 and 46 in lines 41, 43 and 45, respectively, are associated with the respective reservoirs for exercising some control over fluid flow if desired, and allowing the flow of various vapors to be completely cut off, as, for example, for system maintenance or reservoir replacement.
  • Pressure control valves 48, 50 and 52 are provided in lines 41, 43 and 45, respectively, so that the rates of flow of the respective vapors from the reservoirs may be controlled.
  • valves 48, 50 and 52 are of a type which are controlled electromagnetically or by means of a motor. Accordingly, motors 54, 56 and 58 are illustrated as being coupled to the valves and operated by controllers 60, 62 and 64 to cause the flow of vapors from the reservoirs to vary in a desired manner.
  • Mass flow rate transducers 66, 68 and 70 are disposed in flow sensing relationship with lines 41, 43 and 45, respectively. The signals provided by these transducers are applied to the controllers so that the mass flow rates of the vapors can be controlled.
  • Each combination of a pressure control valve, motor, controller and transducer for example those elements represented by numerals 48, 54, 60 and 66, is referred to as a mass flow controller.
  • controllers are conventionally found in fluid flow systems, and various appropriate types of controllers are readily commercially available.
  • One example of such a controller is the Tylon model FC-260, available from the Tylon Corp. of Torrance, California.
  • the motor 54 for example, comprises an electric heater coupled to a differential expansion tube with an attached ball which moves relative to the valve seat to vary the ball-to-seat opening, thus regulating gas flow through the valve.
  • Each of the controllers 60, 62 and 64 has a setpoint input terminal which is connected to the system control unit 72 which may comprise a microprocessor or computer which is programmed to provide each controller with an appropriate control signal.
  • Controller 72 may comprise an A-D converter with a model 3911 A controller, a model 1500 CAMAC crate (Kinetic Systems Inc.) coupled to a PDP 11/34 computer using a VT 52 video terminal, programmer console, DEC writer, RK 11T disk and a software, the last six components being obtainable from Digital Equipment Corporation.
  • Vapor delivery lines 41, 43, 45 and 71 must be heated to a temperature at least as high as the maximum temperature to which reservoirs 18, 20 and 22 are heated.
  • Oxygen may also be introduced into line 71 from a source 74.
  • the rate of oxygen flow is controlled by a mass flow controller comprising valve 76, motor 78, controller 80 and transducer 82.
  • the flow rate of the oxygen is preferably controlled as a function of the flow rate of the vapor constituents so that an appropriate amount of oxygen is introduced into the system.
  • FIG. 1 A fragmentary cross-sectional view of burner 12 is illustrated in Figure 2.
  • a centrally located orifice 86 in burner face 84 is surrounded by concentric rings of orifices 88, 90 and 92.
  • the reactant vapors emanate from orifices 86 where they are subjected to heat from a flame produced by the fuel gas and oxygen emanating from orifices 90.
  • a stream of oxygen, referred to as the inner shield emanates from orifices 88; this stream prevents reaction of the reactant compounds at the burner face.
  • a stream of oxygen referred to as the outer shield emanates from orifices 92.
  • This burner design is somewhat similar to that disclosed in U.S.A. Patent No. 3,698,936 issued to H. J. Moltzan, the Moltzan patent differing in that it teaches an annular slot for providing the inner shield and in that it lacks the outer shield orifices. All of the orifices of burner 12 can be supplied by manifolds similar to those taught in the Moltzan patent.
  • fuel gas and oxygen which are supplied to burner 12 by line 14, issue from the burner and are ignited. Additional oxygen may be supplied by line 15.
  • the reactant vapors supplied by line 71 react in the flame to form a glass soot which is directed toward preform 16.
  • the chlorine or other material with which the matrix and dopant materials had previously been combined is separated from the materials, and combines with hydrogen from the hydrocarbon fuel to form hydrochloric acid.
  • the specific nature of the reaction depends, of course, upon the constituents present and the specific application of the invention. Such reactions themselves form no part of the present invention, and it is anticipated that constituents other than those disclosed herein may be used without departing from the thesis of the invention.
  • deposition apparatus such as the aforementioned IVPO apparatus, or other mechanisms which transfer the matrix and dopant materials to a substrate, may be selected for use with the invention.
  • additional oxygen above and beyond the stoichiometric amount required for combustion of the fuel may be delivered to the burner 12, for example, in the manner described in conjunction with Figure 2.
  • reservoirs 18, 20 and 22 may contain SiCl 4 , GeCI 4 and BCI 3 , respectively.
  • SiCl 4 , GeCI 4 and BCI 3 glassform- ing reactants capable of being delivered in vapor form may be employed.
  • Temperature controllers 30, 32 and 34 are adjusted so that the vapor pressure in the respective reservoirs is sufficiently high to permit the vapors to be delivered through the mass flow controllers to the burner or other utilization means.
  • a minimum pressure of 4 psig. 27 x 10 3 Pascals gauge
  • a constructed embodiment was adjusted so that the pressure within the reservoirs is maintained at about 12 psig. (83 x 10 3 Pascals gauge).
  • the temperature of the SiCl 4 , GeCI 4 and BCI 3 should be maintained at about 76°C, 105°C and 30°C respectively.
  • Valves 42, 44 and 46 are opened and system control 72 provides each of the mass flow controllers with appropriate set point signals so that valves 48, 50 and 52 pass the desired amount of vapor to burner 12.
  • a properly-metered flow of oxygen is also introduced into the burner along with the reactant vapors.
  • the vapors react with oxygen in the flame or form soot which is deposited upon the surface of soot preform 16.
  • Mandrel 10 is removed from the completed preform which is then heated and consolidated into a monolithic glassy blank which can be drawn into an optical waveguide in the conventional manner.
  • system control 72 is caused to produce command signals for various ones of the mass flow controllers at predetermined times so that the amount or kind of dopants are changed.
  • the change is such as to effect a decrease in the refractive index of the ultimate glass product with increasing preform radius. Accordingly, flow control valves 48, 50 and 52 appropriately regulate the flow of reactant vapors therethrough.
  • the disclosed type of vapor delivery system is capable of delivering reactant vapors to a deposition apparatus with extremely high accuracy. Accurate control of the temperature and pressure of the liquids in the reservoirs is unnecessary; it is only necessary to maintain the pressure therein sufficiently high so that the vapors can be transported through the mass flow controllers to the burner.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Optical Integrated Circuits (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Chemical Vapour Deposition (AREA)
  • Glass Compositions (AREA)
  • Physical Vapour Deposition (AREA)
  • Paper (AREA)
  • Auxiliary Devices For And Details Of Packaging Control (AREA)
  • Laser Surgery Devices (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Lubricants (AREA)
  • Fats And Perfumes (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Heating, Cooling, Or Curing Plastics Or The Like In General (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicinal Preparation (AREA)
  • Communication Cables (AREA)
  • Mechanical Coupling Of Light Guides (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Manufacturing Of Printed Wiring (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Control Of Steam Boilers And Waste-Gas Boilers (AREA)
EP80300618A 1979-03-01 1980-02-29 Adjustable vapour deposition apparatus Expired EP0018068B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT80300618T ATE10292T1 (de) 1979-03-01 1980-02-29 Regelbare aufdampfquelle.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/016,446 US4314837A (en) 1979-03-01 1979-03-01 Reactant delivery system method
US16446 1979-03-01

Publications (2)

Publication Number Publication Date
EP0018068A1 EP0018068A1 (en) 1980-10-29
EP0018068B1 true EP0018068B1 (en) 1984-11-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP80300618A Expired EP0018068B1 (en) 1979-03-01 1980-02-29 Adjustable vapour deposition apparatus

Country Status (15)

Country Link
US (1) US4314837A (es)
EP (1) EP0018068B1 (es)
JP (1) JPS55116640A (es)
AT (1) ATE10292T1 (es)
AU (1) AU517154B2 (es)
BR (1) BR8001187A (es)
CA (1) CA1136402A (es)
DE (1) DE3069619D1 (es)
DK (1) DK154416C (es)
ES (1) ES489018A0 (es)
FI (1) FI67361C (es)
IL (1) IL59484A (es)
IN (1) IN152644B (es)
NO (1) NO147416C (es)
YU (1) YU56880A (es)

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JP5023016B2 (ja) * 2007-08-10 2012-09-12 信越化学工業株式会社 光ファイバ製造装置および線引き炉のシール方法
US10464838B2 (en) 2015-01-13 2019-11-05 Asi/Silica Machinery, Llc Enhanced particle deposition system and method
JP6793676B2 (ja) 2018-04-02 2020-12-02 信越化学工業株式会社 光ファイバ用多孔質ガラス母材の製造装置および製造方法
JP7155075B2 (ja) * 2019-07-31 2022-10-18 株式会社フジクラ 光ファイバの製造方法
JP7449842B2 (ja) * 2020-11-02 2024-03-14 信越化学工業株式会社 多孔質ガラス母材の製造方法及び製造装置
JP7428632B2 (ja) 2020-12-14 2024-02-06 信越化学工業株式会社 多孔質ガラス母材の製造方法及び製造装置

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FI800604A (fi) 1980-09-02
NO147416B (no) 1982-12-27
JPS6320772B2 (es) 1988-04-30
DK85880A (da) 1980-09-02
ES8103386A1 (es) 1981-02-16
IL59484A (en) 1985-01-31
AU5596180A (en) 1980-09-04
DK154416C (da) 1989-05-16
NO800571L (no) 1980-09-02
EP0018068A1 (en) 1980-10-29
DE3069619D1 (en) 1984-12-20
YU56880A (en) 1983-09-30
ES489018A0 (es) 1981-02-16
BR8001187A (pt) 1980-11-04
FI67361B (fi) 1984-11-30
ATE10292T1 (de) 1984-11-15
DK154416B (da) 1988-11-14
CA1136402A (en) 1982-11-30
AU517154B2 (en) 1981-07-09
JPS55116640A (en) 1980-09-08
FI67361C (fi) 1985-03-11
IN152644B (es) 1984-03-03
NO147416C (no) 1984-03-21
IL59484A0 (en) 1980-05-30
US4314837A (en) 1982-02-09

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